WO2020062008A1 - Verre optique de fluorophosphate et préforme, élément et instrument optiques - Google Patents

Verre optique de fluorophosphate et préforme, élément et instrument optiques Download PDF

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Publication number
WO2020062008A1
WO2020062008A1 PCT/CN2018/108273 CN2018108273W WO2020062008A1 WO 2020062008 A1 WO2020062008 A1 WO 2020062008A1 CN 2018108273 W CN2018108273 W CN 2018108273W WO 2020062008 A1 WO2020062008 A1 WO 2020062008A1
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WO
WIPO (PCT)
Prior art keywords
glass
optical glass
fluorophosphate
optical
fluorophosphate optical
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PCT/CN2018/108273
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English (en)
Chinese (zh)
Inventor
孙伟
Original Assignee
成都光明光电股份有限公司
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Publication date
Application filed by 成都光明光电股份有限公司 filed Critical 成都光明光电股份有限公司
Priority to PCT/CN2018/108273 priority Critical patent/WO2020062008A1/fr
Priority to JP2021517199A priority patent/JP2022502333A/ja
Priority to US17/279,575 priority patent/US20210395135A1/en
Priority to KR1020217008806A priority patent/KR102608946B1/ko
Priority to EP18934652.1A priority patent/EP3858796B1/fr
Publication of WO2020062008A1 publication Critical patent/WO2020062008A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/23—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
    • C03C3/247—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron containing fluorine and phosphorus
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/04—Prisms
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
    • C03B11/06—Construction of plunger or mould
    • C03B11/08—Construction of plunger or mould for making solid articles, e.g. lenses
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2215/00—Press-moulding glass
    • C03B2215/40—Product characteristics
    • C03B2215/41—Profiled surfaces
    • C03B2215/412—Profiled surfaces fine structured, e.g. fresnel lenses, prismatic reflectors, other sharp-edged surface profiles
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements

Definitions

  • the invention belongs to the technical field of optical glass, and specifically relates to a fluorophosphate optical glass, an optical prefabricated part, an element and an instrument.
  • Fluorophosphate optical glass is a new glass material with low refractive index and low dispersion. It can eliminate special dispersion of the secondary spectrum in the optical system, improve resolution, improve the imaging quality of the optical system, and also has low softening properties. It can be directly precision-molded into aspheric lenses, which can better eliminate chromatic aberration, spherical aberration, aberration, and reduce system volume and weight.
  • fluorophosphate optical glass has been widely used in high-precision, high-resolution optical instrument combination lenses such as digital cameras, high-definition surveillance, astronomical telescopes, and has become a new type of optoelectronic material with potential market prospects. Specific applications in these fields place higher requirements on the performance of fluorophosphate optical glass.
  • fluorophosphate optical glass with an Abbe number of 80 or greater, but these fluorophosphate Salt optical glass has high density, poor chemical stability and anti-crystallization performance, high thermal expansion coefficient, low bubble level, and is easy to cause damage during molding and heating.
  • the object of the present invention is to provide a fluorophosphate optical glass, an optical preform, an element and an instrument having a refractive index (nd) of 1.42-1.45 and an Abbe number (vd) of 93-96.
  • the fluorophosphate optical glass of the present invention has low density, excellent chemical stability and anti-crystallization performance, low coefficient of thermal expansion, low breakage during molding and thermal processing, high level of air bubbles, and can realize stable mass production.
  • fluorophosphate optical glass the cation contains P 5+ , Al 3+ and alkaline earth metal ions, and the anion contains F - and O 2- ;
  • the thermal expansion coefficient of the optical glass ⁇ 20 ° C -120 ° C ) is 160 ⁇ 10 -7 / K or less; density ( ⁇ ) is 3.55 g / cm 3 or less; water resistance stability (D w ) is 2 or more.
  • Fluorophosphate optical glass contains P 5+ : 2-20%, Al 3+ : 20-40%, Ba 2+ : 0.5-10%, Sr 2+ : 5-25%, Ca 2 +: 15-35%, Mg 2+: 1-15%; anion mole percent, containing F -: 83-95%, O 2- : 5-17%.
  • Ln 3+ 0-6%, Na + : 0-10%, Li + : 0-10%, K + : 0-10%, where Ln 3+ is La 3+ , Gd 3+ , Y 3+ and Yb 3+ .
  • Fluorophosphate optical glass calculated by cation molar percentage from P 5+ : 2-20%, Al 3+ : 20-40%, Ba 2+ : 0.5-10%, Sr 2+ : 5-25%, Ca 2 + : 15-35%, Mg 2+ : 1-15%, Na + : 0-10%, Li + : 0-10%, K + : 0-10%, Ln 3+ : 0-6%, 3+ 3+ in LN of one or more of La 3+, Gd 3+, Y 3+ and Yb, anionic mole percent, the F -: 83-95%, O 2- : 5-17% composition.
  • the refractive index (nd) of the glass is 1.42-1.45, preferably 1.43-1.44; the Abbe number (vd) is 93-96, preferably 94-95.5.
  • Ba 2+ / Ca 2+ is 0.01-0.155
  • / or Ba 2+ / (Ca 2+ + Mg 2+ ) is 0.08-0.13
  • / or O 2- / F - is 0.105-0.2 .
  • Ba 2+ / Ca 2+ is 0.05-0.155
  • / or Ba 2+ / (Ca 2+ + Mg 2+ ) is 0.09-0.125
  • / or O 2- / F - is 0.11-0.18 .
  • Ba 2+ / Ca 2+ is 0.1-0.15
  • / or Ba 2+ / (Ca 2+ + Mg 2+ ) is 0.1-0.12
  • / or O 2- / F - is 0.11-0.15 .
  • Y 3+ 0-5%, preferably 0-4%, more preferably 0.5-3%
  • La 3+ 0-5%, preferably 0-3%, more preferably 0-1 %
  • Gd 3+ 0-5%, preferably 0-3%, more preferably 0-1%
  • Yb 3+ 0-5%, preferably 0-3%, more preferably 0-1%.
  • the coefficient of thermal expansion ( ⁇ 20 ° C-120 ° C ) of the glass is 155 ⁇ 10 -7 / K or less; the density ( ⁇ ) is 3.53 g / cm 3 or less; the degree of air bubbles is B or higher, preferably A or higher, more It is preferably A 0 or higher; the water resistance stability (D w ) is 1 or higher.
  • Optical element made of the above-mentioned fluorophosphate optical glass and optical preform.
  • the present invention has the following beneficial effects:
  • the fluorophosphate optical glass of the present invention has excellent chemical stability, anti-crystallization performance, coefficient of thermal expansion, and bubble degree.
  • the refractive index (nd) of the fluorophosphate optical glass of the present invention is 1.42-1.45, Abbe number (vd) is 93-96, thermal expansion coefficient ( ⁇ 20 °C -120 °C ) is 160 ⁇ 10 -7 / K or less; density ( ⁇ ) is 3.55g / cm 3 or less; bubble degree is B grade or higher; water resistance
  • the operational stability (D w ) is 2 or more.
  • each cationic component and the cationic component is represented by “molar percentage of cation”
  • the total content of each anionic component and anionic component is represented by “anionic mole percentage”.
  • the "molar percentage of cations” refers to the percentage of the molar content of a certain cationic component
  • the “molar percentage of anions” refers to the percentage of the molar content of an anionic component.
  • the ionic valence of each component is only a representative value used for convenience, and is not different from other ionic valences.
  • the ion valence of each component present in the optical glass may be other than the representative value.
  • P generally exists in glass in a state where the ionic valence is 5 valences. Therefore, "P 5+ " is used as a representative in this specification, but there is a possibility that it exists in other ionic valence states. Within the scope of protection.
  • P 5+ is an important component that plays a role as a network structure in fluorophosphate glass. It and O 2- together form the main element of the glass skeleton, which can effectively improve the mechanical properties of the glass while maintaining the glass forming stability.
  • the fluorophosphate optical glass of the present invention when the content of P 5+ is less than 2%, the crystallization tendency of the glass is increased, and the stability is deteriorated; when the content of P 5+ is more than 20%, The performance is greatly affected, and it is difficult to obtain the optical constants required by the present invention. Therefore, in order to balance the stability and optical performance of glass, the content of P 5+ is limited to 2-20%, preferably 3-15%, and more preferably 5-10%.
  • Al 3+ is an important component for improving devitrification resistance and chemical stability in fluorophosphate glass.
  • the lower limit is 20%, preferably 25%. More preferably, it is 30%; when the content is higher than 40%, the required refractive index and Abbe number cannot be obtained due to the reduction of the content of other components, and the glass transition temperature Tg will increase significantly, resulting in an increase in molding temperature and milk. The turbidity tendency increases, the brittleness increases, and the degree of abrasion increases. Therefore, the upper limit of the content of Al 3+ is 40%, preferably 38%, more preferably 37%, still more preferably 36%, and still more preferably 35%.
  • the main role of Ba 2+ , Sr 2+ , Ca 2+ , Mg 2+ and other alkaline earth metals is to improve the chemical stability and anti-crystallization of the glass, make the glass achieve the expected optical properties, control the refractive index and Abbe number, At the same time, it can optimize the production process of optical glass.
  • Ba 2+ is beneficial to improve the devitrification resistance and refractive index of the glass.
  • the content of Ba 2+ is limited to 0.5-10%, preferably 1-8%, and more preferably 1-5%.
  • Sr 2+ is effective for improving the devitrification resistance of the glass, and can effectively adjust the refractive index and specific gravity of the glass. If the content is too large, the refractive index and dispersion of the glass will be increased, and it is difficult to achieve the expected optical properties. Will reduce the chemical stability of the glass. Therefore, in order to obtain better optical performance, the content of Sr 2+ is limited to 5-25%, preferably 10-22%, and more preferably 15-20%.
  • Ca 2+ can reduce the Abbe number and specific gravity of glass, stabilize the formation of glass, improve the acid resistance and abrasion resistance of glass. If its content is too low, it will not reach the required optical properties. If its content is too high, the glass will have devitrification resistance. And the chemical stability deteriorates. Therefore, the content of Ca 2+ is limited to 15-35%, preferably 20-333%, and more preferably 25-30%.
  • Mg 2+ has the effect of improving the thermal stability and abrasion resistance of glass. It is added to effectively improve the glass forming property, devitrification resistance and processability of glass. If its content is too low, the processability adjustment will be low and increase. Glass processing is difficult. If the content is too high, the content of other alkaline earth metals will be reduced, and the required optical properties will not be achieved. Therefore, the content of Mg 2+ is limited to 1-15%, preferably 2-12%, and more preferably 5-10%.
  • the inventors researched and found that when the four alkaline earth metals (Ba 2+ , Sr 2+ , Ca 2+ , Mg 2+ ) were added in synergy, the properties of the glass were adjusted together. Only when the refractive index and Abbe number of the fluorophosphate optical glass of the present invention are obtained, the glass has good chemical stability (including water resistance stability and acid resistance stability), bubble degree grade and anti-crystallization performance, and at the same time, molding And heating is not easy to break, reducing the difficulty of production process.
  • the ratio of Ba 2+ / Ca 2+ is higher than 0.155, the specific gravity of the glass increases, and it is difficult to achieve the purpose of weight reduction.
  • the ratio of Ba 2+ / Ca 2+ is less than 0.01, the glass is prone to generate bubbles. Degradation resistance.
  • Ba 2+ / Ca 2+ is limited to 0.01-0.155, preferably 0.03-0.155, It is more preferably 0.05-0.155, and still more preferably 0.1-0.15.
  • Ba 2+ / (Ca 2+ + Mg 2+ ) When the ratio of Ba 2+ / (Ca 2+ + Mg 2+ ) is higher than 0.13, the addition of Ba 2+ , Ca 2+ , and Mg 2+ is unbalanced, and the specific gravity of the glass increases; when Ba 2+ / ( When the ratio of Ca 2+ + Mg 2+ ) is less than 0.08, the chemical stability of the glass is deteriorated, and the anti-crystallization performance is decreased. Therefore, in order to reduce the density of the glass, improve the chemical stability of the glass and the anti-crystallization performance, Ba 2+ / (Ca 2+ + Mg 2+ ) is limited to 0.08-0.13, preferably 0.09-0.125, and more preferably 0.1- 0.12.
  • Alkali metals Li + , Na +, and K + can reduce the viscosity of glass, the glass transition temperature, and the components of glass that are easy to manufacture, but excessive introduction will reduce the stability, cause the glass's thermal expansion coefficient to increase, and water resistance stability to decrease. Therefore, the content of Na + is limited to 0-10%, preferably 0-4%, and more preferably 0.5-2%; the content of Li + is limited to 0-10%, preferably 0.5-5%, and more preferably 0.5 -3%; The content of K + is limited to 0-10%, preferably 0-5%, more preferably 0-2%, and still more preferably no introduction.
  • Ln 3+ (La 3+ , Gd 3+ , Yb 3+ , Y 3+ ) as a rare earth element is a component that maintains the low dispersion of the glass and increases the refractive index.
  • the content is too high to achieve the above effects, but it is excessive. Addition will cause the refractive index of the glass to exceed the required range, while increasing the melting temperature and reducing the chemical stability of the glass. Therefore, the total content of the rare earth element Ln 3+ is limited to 0-6%, preferably 0-5%, and more preferably 0.5-3%.
  • Y 3+ 0-5%, preferably 0-4%, more preferably 0.5-3%; La 3+ : 0-5%, preferably 0-3%, more preferably 0-1%; Gd 3+ : 0-5%, preferably 0-3%, more preferably 0-1%; Yb 3+ : 0-5%, preferably 0-3%, more preferably 0-1%.
  • the cations of Pb, Th, Cd, Tl, Os, Be, and Se have tended to be used as harmful chemicals in recent years. They not only protect the environment from the glass manufacturing process to the processing process and disposal after productization. The measures are required. Therefore, in a case where the impact on the environment is valued, it is preferable that they are not actually contained except for unavoidable mixing. As a result, the optical glass becomes practically free of substances that pollute the environment. Therefore, the optical glass of the present invention can be manufactured, processed, and discarded without taking special environmental measures.
  • O 2- and F - are anionic components, which are added to achieve the required optical performance and glass stability.
  • F - is a key component that makes the glass have low dispersion and abnormal dispersion. It has an effect on reducing the refractive index temperature coefficient and T g . If its content is too low, it will be difficult to achieve the required performance; if its content is too high, it will Weaken the chemical stability of glass, increase the coefficient of thermal expansion and abrasion, especially during the melting process, the volatility of F will not only pollute the environment, but also make the internal composition of the glass uneven, causing defects such as abnormal data and stripes. Accordingly, the content of F - is limited to 83-95%, preferably 85-92%, more preferably 87-91%.
  • O 2- is an essential component that constitutes a fluorophosphate optical glass network structure. Its content is too low, glass stability is poor, and it is difficult to achieve the refractive index required by the present invention. Too high content is difficult to obtain the required dispersion and abnormal dispersion. Therefore, the content of O 2- is limited to 5-17%, preferably 8-15%, and more preferably 9-13%.
  • O 2- / F When the ratio of-is lower than 0.105, the thermal expansion coefficient of the glass is higher, and the moldability is poor.
  • the ratio of O 2- / F- is higher than 0.2, the glass forming performance is not favorable. Therefore, in order to reduce the coefficient of thermal expansion of the glass, make molding and hot working difficult to break, and improve the glass forming performance, the ratio of O 2- / F- is limited to 0.105-0.2, preferably 0.11-0.18, and more preferably 0.11-0.15.
  • the anion may contain Cl ⁇ , and Cl ⁇ may be introduced in the form of a chloride of the above cation, preferably in the form of BaCl 2.
  • Cl ⁇ may be introduced in the form of a chloride of the above cation, preferably in the form of BaCl 2.
  • its content is 0-1%.
  • the refractive index (nd) and Abbe number (vd) are tested according to the GB / T7962.1-2010 test method.
  • the thermal expansion coefficient ( ⁇ 20 °C -120 °C ) is tested according to the GB / T7962.16-2010 test method.
  • the density ( ⁇ ) is tested according to the GB / T7962.20-2010 test method.
  • the bubble degree is tested according to the GB / T7962.8-2010 test method.
  • D W Water resistance stability
  • the test method for the anti-crystallization performance of the glass in the present invention is: cut the sample glass into 20 ⁇ 20 ⁇ 10mm specifications, and place it in a muffle furnace with a temperature of T g + 230 ° C for a preset temperature of 30 minutes. The insulation cotton was cooled slowly. After cooling, the surface crystallization was observed with the naked eye. No obvious crystallization was recorded as "A”, and obvious crystallization was recorded as "B".
  • the fluorophosphate optical glass provided by the present invention has the following properties:
  • Refractive index (nd) is 1.42-1.45, preferably 1.43-1.44; Abbe number (vd) is 93-96, preferably 94-95.5; density ( ⁇ ) is 3.55 g / cm 3 or less, preferably 3.53 g / cm 3 or less; bubble of class B or more, preferably above A, more preferably A level 0; coefficient of thermal expansion ( ⁇ 20 °C -120 °C) of 160 ⁇ 10 -7 / K or less, preferably 155 ⁇ 10 - 7 / K or less.
  • the melting and forming method for producing optical glass may employ a technique known to those skilled in the art.
  • the glass raw materials carbonate, nitrate, metaphosphate, fluoride, oxide, etc.
  • a melting device such as a platinum crucible
  • 900 ⁇ 1250 °C After proper stirring, clarification, and homogenization, the temperature is lowered to below 900 °C, poured or missed into the forming mold, and finally subjected to post-treatment such as annealing and processing, or directly pressed by precision molding technology.
  • the fluorophosphate optical glass of the present invention can be used as a glass preform for pressure molding, or the molten glass can be directly pressure molded.
  • the manufacturing method and the thermoforming method used as a glass preform are not specifically limited, A well-known manufacturing method and a shaping method can be used.
  • the present invention also provides an optical element, which is formed from the above-mentioned optical glass according to a method well known to those skilled in the art, such as directly performing pressure processing on the molten and softened optical glass to manufacture the optical element.
  • the glass preform made of the optical glass of the present invention is subjected to pressure processing to manufacture an optical element.
  • the invention also provides an optical instrument, which is manufactured by using the optical element manufactured as described above.
  • an optical instrument which is manufactured by using the optical element manufactured as described above.
  • biconvex, biconcave, plano-convex, plano-concave, concave-convex lenses and other lenses, mirrors, prisms, diffraction gratings, etc. can be applied to digital cameras, digital video cameras, camera phones and other equipment.
  • composition and refractive index (nd), Abbe number (vd), density ( ⁇ ), bubble degree, thermal expansion coefficient, and water resistance stability of the fluorophosphate optical glass of Examples 1-37 and Comparative Examples 1-3 of the present invention ( The results of D w ) and the anti-crystallization performance are shown in Tables 1-4, and the components of each component are expressed in mol%.
  • the optical glass obtained in Example 1-37 was cut into a predetermined size, and a release agent was evenly coated on the surface, and then it was heated, softened, and pressure-molded to produce a concave meniscus lens and a convex meniscus.
  • the optical glass obtained in Example 1-37 is used to form a preform for precision press molding, and then precision press molding is performed into the shape of a lens and a prism to produce a preform.
  • the preforms obtained in the foregoing embodiments of the optical preforms are annealed, and fine adjustment is performed while reducing the deformation inside the glass, so that the optical properties such as the refractive index reach the desired value.
  • each preform is ground and ground to produce various lenses and prisms such as a concave meniscus lens, a convex meniscus lens, a biconvex lens, a biconcave lens, a plano-convex lens, and a plano-concave lens.
  • An anti-reflection film may be coated on the surface of the obtained optical element.
  • the optical element prepared by the above-mentioned optical element embodiment is designed by optical design, and an optical component or an optical component is formed by using one or more optical elements, which can be used in, for example, imaging equipment, sensors, microscopes, medical technology, digital projection, communication, and optical communication.

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Abstract

L'invention concerne un verre de fluorophosphate, et une préforme, un élément et un instrument optiques, se rapportant au domaine technique du verre optique. Le verre optique contient les constituants suivants, en pourcentage molaire de cations : P5+ : 2-20 %, Al3+ : 20-40 %, Ba2+ : 0,5-10 %, Sr2+ : 5-25 %, Ca2+ : 15-35 % et Mg2+ : 1-15 % et contient les constituants suivants en pourcentage molaire d'anions : F- : 83-95 % et O2- : 5-17 %. Le verre optique de fluorophosphate présente un indice de réfraction (nd) de 1,42-1,45, un nombre d'Abbe (vd) de 93-96, une densité (ρ) de 3,55 g/cm3 ou moins, un degré de bulle de grade B ou plus, un coefficient de dilatation thermique de 160×10-7/K ou moins, une stabilité de résistance à l'eau (Dw) de type 2 ou plus et d'excellentes propriétés anticristallisation.
PCT/CN2018/108273 2018-09-28 2018-09-28 Verre optique de fluorophosphate et préforme, élément et instrument optiques WO2020062008A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
PCT/CN2018/108273 WO2020062008A1 (fr) 2018-09-28 2018-09-28 Verre optique de fluorophosphate et préforme, élément et instrument optiques
JP2021517199A JP2022502333A (ja) 2018-09-28 2018-09-28 フルオロリン酸光学ガラス、並びに光学プリフォーム、素子、及び機器
US17/279,575 US20210395135A1 (en) 2018-09-28 2018-09-28 Fluorophosphate optical glass, and optical preform, element and instrument
KR1020217008806A KR102608946B1 (ko) 2018-09-28 2018-09-28 플루오로포스페이트 광학 유리, 광학 프리폼, 소자 및 기기
EP18934652.1A EP3858796B1 (fr) 2018-09-28 2018-09-28 Verre optique de fluorophosphate et préforme, élément et instrument optiques

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PCT/CN2018/108273 WO2020062008A1 (fr) 2018-09-28 2018-09-28 Verre optique de fluorophosphate et préforme, élément et instrument optiques

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CN101665326A (zh) * 2008-09-04 2010-03-10 Hoya株式会社 碎玻璃原料的制造方法、氟磷酸玻璃的制造方法
CN101665324A (zh) * 2008-09-04 2010-03-10 Hoya株式会社 氟磷酸玻璃的制造方法
CN102300823A (zh) * 2009-08-26 2011-12-28 Hoya株式会社 氟磷酸盐玻璃、模压成型用玻璃材料、光学元件坯料、光学元件及其制造方法和玻璃成型体的制造方法

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CN112707640A (zh) * 2021-01-21 2021-04-27 成都光明光电股份有限公司 氟磷酸盐光学玻璃、光学元件及光学仪器
IT202100003530A1 (it) 2021-02-16 2022-08-16 Angelantoni Test Tech S R L In Breve Att S R L Fluido refrigerante

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